烟草科技Issue(4)：37-43,7.
LC-MS/MS测定尿液中的11种多环芳烃生物标志物
Determination of 11Polycyclic Aromatic Hydrocarbon Biomarkers in Human Urine with LC-MS/MS
摘要
Abstract
In order to evaluate the exposure to PAHs in environmental tobacco smoke, the influences of solid phase extraction column, chromatographic column and mass spectrometry conditions on analytical results were investigated, a method with SPE-HPLC/MS/MS was established to determine the biomarkers of 1-OHNap, 2-OHNap, 1-OHPyr, 6-OHChr, 3-OHFlu, 1-OHPhe, 2-OHPhe, 3-OHPhe, 4-OHPhe, 9-OHPhe and 2-OHFlu in human urine. Using l-OHNap-d8, 3-OHPhe-d9 and l-OHPyr-d9 as internal standards, the samples were hydrolyzed by ?-glucosidase/aryl sulfatase, extracted by Bond Elut C18 cartridge, separated by Eclipse PAH column, determined by mass spectrometry under multi-reaction monitoring mode (MRM), the OH metabolites of PAHs (OHPAHs) in urine were detected. The results showed that the limits of quantification (LOQ) of OHPAHs varied from 6 to 130 pg/mL. The detectable concentration of OHPAHs showed good linear relationship with r from 0.9991 to 1.0000, and the recoveries ranged from 72.45% to 124.50%. The intra-day and inter-day precisions were in the range of 1.49% to 7.35% and 2.90% to 12.00%, respectively. This method is suitable for simultaneously determining the biomarkers of PAHs in human urine.关键词
尿液/多环芳烃/生物标志物/液相色谱-串联质谱/多反应监测模式(MRM)Key words
Urine/ PAH/ Biomarker/ LC-MS/MS/ Multi-reaction monitoring mode (MRM) .分类
轻工纺织引用本文复制引用
陈玉松,王昇,余晶晶,刘惠民,曹德坡..LC-MS/MS测定尿液中的11种多环芳烃生物标志物[J].烟草科技,2012,(4):37-43,7.基金项目
郑州烟草研究院科技项目“卷烟烟气多生物标志物检测研究”(322010CZ0590). （322010CZ0590）
